IndicatorFunnel Nozzle

VacuumFlange

Filter

Filter

pump

pumppump

pump

gas

Pressure Gauge

VacuumGauge

Reservo

ir

Sup

ply

Ves

sel

Burst Disk

Tank

Vdrain

liquid

exhaust

Vtransfer Vnozzle Vgas-manifold

Vblocking

Vthree-way

Vprotect

Vbypass

Vevac-tank

Vevac-line

Csupply-drain

Creservoir-drain

CfunnelCaux

COLTRIMS LIQUID-TO-GAS MANIFOLD

op

tio

nal

gas

& li

qu

id s

up

ply

Caps (screw on)

ValvesFillingFunnel

Cdry-outVDry-out

Vseed

Vpump

Vexhaust

Knee

drainCexhaust

VsupplyVsyringe

CheckValve

HOW LONG WILL 100ml (OF WATER) LAST ?

We assume the following:Volume = 100mlPressure = 100psiNozzle = 30micronsTurbo pumping speed = maximum ~1400 l/s for N2 – we guess ~1000 l/s for water (Note: only below ~7.5E-4 Torr most turbo pumps operate at their maximum pump capacity)

Assume that the gas expands into 4E-4 Torr (0.0532Pa) pressure and that this pressure is stable. This implies that the pump removes at most 1000 l/s of 4E-4 Torr pressure (water) gas. In this pressure regime the amount of gas produced by a substance is given by: PV=nRT. R =8.3144621 J/(K*mol), T = 373 K, n = 100*p/(molar mass) (for water this is 100g/(18 g/mol) = 5.5 mol), P = 0.0532 Pa. With these values we get V = 320,623 m^3 = 3.21E8 l.

Divide V by the pump speed to get 321,000 s. Divide by 3600 s to get hours:Duration minimum = 89.16 hrs (Water). Divide by 24 hrs to get days:Duration minimum = 3.7 days (Water).

To get the pump time for your liquid, find the number of moles m in the liquid reservoir and multiply this number by m/5.5.

2

PUMP DOWN OF THE DRY LIQUID-TO-GAS MANIFOLD: Start-up Phase

Preparation !!!In case you need to evacuate the >>tank<< make sure you have the valve Vevac-tank open during the pump down of the chamber. If you forgot to evacuate during the pump down phase you need to make sure that the “hidden bypass” and the bypass between the chamber and the 2nd stage is closed; open Vevac-tank very slowly.

Get the Liquid-to-Gas Manifold ready1. Close Vdrain

2. Close Caux

3. Close and lock Vtransfer

4. Close and lock Vgas-manifold

5. Close Creservior-drain or Vseed and Vsupply in case you use the optional liquid and gas supply arm6. Close Caux

7. Close Vbypass

8. Close Vprotect

9. Open Vblocking

10. Open Vevac-line

Start “chem-lab” diaphragm pump in controller rack11. Open Vthree-way to pump12. Pump for 1 minute13. Open Vnozzle

14. Pump for 1 minute and check Pressure Gauge (should go down)15. Close Vthree-way

Make sure the chamber fore-vacuum is running (especially scroll at 2nd stage)16. Open Vbypass slowly only when the manifold and the reservoirs are dry !17. Open Vprotect

18. Let it pump for 10 minutes 3

START/STOP HEATING

INSIDE THE CHAMBER

Use heat controller on Controller RackHeat the gas line firstset desired temperature to 120deg C: DO NOT GO HIGHER IN TEMPERATURE !!!• turn on controller unit (switch in the back)• select thermocouple and temperature units (1.: press “” for 3 sec. , press “” till you get “Inpt”, press “”

or “” till you get “J”, only if “J” is flashing hit “”. 2.: Press “” till you get “tpun”, press “” or “” till you get “C”, only if “C” is flashing hit “”. )

• enable PID mode (press “” till you get “ctrl”, press “” or “” till you get “PID”; only if “PID” is flashing hit “”)

• set desired temperature (press “”, press “” or “” and then confirm with “”) • turn on the heater controller (flick the switch labeled “heater controller on” up; check if fans are running)• start PID controller (press “” till you get “r-S”, press “” or “” till you get “run”, only if “run” is flashing

hit “”)• set digital trimmer to restrict max. current (set dip switch to “10” to “15”, i.e. 10 to 15% of 5A; the lower the

better! Recommended: “10” for nozzle and “13” for gasline)

Heat the nozzle nextset desired temperature to 125deg C: DO NOT GO HIGHER IN TEMPERATURE !!!=> see instructions above

To stop heating: - stop PID controller (press “” till you get “r-S”, press “” or “” till you get “stop”, if flashing hit “”)- set digital trimmer to restrict min. current (set dip switch to “00”)

See page 8 for the heating outside the chamber4

MAKE A LIQUID-TO-GAS JET

Prepare the Chamber1. Close all chamber bypasses2. Set Vacuum Gauge controller to appropriate ranges

(Jet Dump: 1E-7, Chamber: 1E-7, 2nd Stage: 1E-6, Source: 1E-4)

Prepare the Liquid-to-Gas Manifold3. Reservoir Heater should be cold (set it to 20deg C); remove sleeve & cool it down with a “water bucket” if

needed;. Note: you cannot and should not transfer liquid into the hot reservoir (safety issue !). 4. Close Vnozzle

5. Close Vprotect

6. Close Vblocking

7. Close Vthree-way

8. Close and lock Vevac

9. Close Vseed

10. Close Vsupply

Option A to fill the Reservoir: Prepare the Transfer Arm of the Manifold11. Close Vtransfer

12. Close Caux

13. Close Csupply-drain

14. Open Vdrain

15. Wear your Personal Protective Equipment (Gloves, Glasses etc.): Fill liquid into small metal funnel slowly to avoid bubbles which can clog the filling mechanism; stop when liquid reaches desired level in glass indicator funnel.

16. Close Vdrain

Transfer the Liquid17. Open Vtransfer slowly and watch the level in the glass indicator funnel drop to desired level18. Close and lock Vtransfer

See next page for Option B to fill the Reservoir => 5

Option B to fill the Reservoir: Prepare and use the Syringe11. Close and lock Vtransfer

12. Wear your Personal Protective Equipment (Gloves, Glasses etc.): Attach the needle to the syringe and suck the (toxic or hazardous) liquid (150ml max) from a beaker in a fume hood.

13. Close Vsyringe and detach the needle14. Connect Syringe assembly to Vsupply (pink nut)

Pump out the connector between Vsupply and Vsyringe

15. Open Vblocking

16. Open Vevac-line

17. Open Vthree-way to the diaphragm forepump18. Pump down for 10 seconds and check Pressure Gauge (should go down)19. Close Vthree-way

20. Close Vevac-line

21. Close Vblocking

Transfer the Liquid17. Open Vsyringe and slowly press the plunger of the syringe down to the desired milliliter value18. Close Vsyringe

19. Close Vsupply

20. The syringe may be disconnected at Vsupply (pink nut); if so cap Vsupply

See next page for instruction how to start the jet =>

6

continue: MAKE A LIQUID-TO-GAS JET

Make a (cold) jet1. Open Vblocking

2. Open Vnozzle slowly (2 to 3 seconds)

Flush out the gasline when needed (when seeding a buffer gas may be used instead: see Seeded Jet section):3. Close Vblocking

4. Open Vevac-line

5. Open Vthree-way to exhaust for 3 seconds6. Open Vthree- way to the forepump and pump for 3 seconds (not longer to avoid water pollution of the pump !)7. Close Vthree-way

8. Close Vevac-line

9. Open Vblocking

10. Start outside Heaters (set to desired temperatures; for the reservoir it is 170deg C max. It is recommended to go up in steps like 50, 80, 100, 120, 150, 170deg C): see next page for instructions

11. Watch the vacuum gauges at the controller rack

7

START/STOP HEATING - continue

OUTSIDE THE CHAMBER

Use heat controllers next to Gas ManifoldHeat the gas line firstset desired temperature to max 125deg C: DO NOT GO HIGHER IN TEMPERATURE !!!• first press the “reset” button on the yellow GFCI plug to supply 110VAC• turn on the unit (red button)• watch out: Unit may immediately starts running if somebody didn’t dial it down before – act fast to stop it• (unit is preset to deg C units and J thermocouples)• select your heating temperature (1.: press ””, 2.: change red value with “” or “”, 3: confirm with “”, 4:

leave menu with pressing ”” twice)

Heat the reservoir nextKeep it cold for the transfer of the liquid; you cannot and should not transfer liquid into the hot reservoir (safety issue !). Set to desired temperature after transfer (165deg C max). It is recommended to go up in steps like 50, 80, 100, 120, 150, 165 deg C…=> see instructions above

To stop heating:- put temperature to “20” temperature (1.: press ””, 2.: change red value with “” or “”, 3: confirm with

“”, 4: leave menu with pressing ”” twice)- verify that the heating stops and the temperature goes down- turn off the unit (red button) - press the “test” button on GFCI plug to cut the AC power

8

STOP AND START JET IN VACUUM CHAMBER

Stop the Jet1. Close Vblocking

2. Open Vevac-line

3. Open Vthree-way to exhaust slowly (should take 3 seconds)4. Open Vthree-way to diaphragm pump and pump for 10 seconds (not longer since condensables are bad for the

diaphragm pump) , then close Vthree-way again5. Do NEVER pump wet reservoir or gas lines via the bypass to the second stage (it will pollute and damage

the scroll forepump).

Restart the Jet1. Close Vthree-ways

2. Close Vevac-line

3. Open Vblocking

9

SEED JET WITH NOBLE GAS: USE OF THE OPTIONAL GAS SUPPLY SYSTEM

Prepare the Gas Supply System1. The reservoir should be empty and dry and cold2. Connect the diaphragm pump to gas supply system3. Close Vblocking and Vtransfer

4. Open Cdrain and connect gas supply system to reservoir5. Connect the gas supply system to the regulator of the gas bottle6. Close Vexhaust

7. Open Vseed, any valves in front of the gas regulator, and the regulator itself to pump to the main valve of the bottle (which should beclosed)

8. Open Vpump and pump for 5 minutes

Make a seeded Jet9. Close Vseed, Vpump, and the regulator (keep any valve in front of the regulator open)10. see MAKE A LIQUID-TO-GAS JET11. Note: It is recommended to start with a low reservoir temperature after the liquid transfer like 50deg C and observe the vacuum

gauges12. To avoid the liquid being pushed through the nozzle apply He buffer gas with a pressure that is higher than the seed gas via Cdry-out:

Open Vdry-out to dial in the pressure while Vevac-line and Vnozzle are open after this section has been pumped out; note the ion gauges need to be preset for this jet. Now open Vblocking and close Vevac-line.

13. Open the gas bottle and dial in a pressure of ~30 to 50 psi. Then open Vseed and watch the gauges. Wait for the He to get out (~10 to 15 minutes)

14. Increase temperature of the liquid and pressure of the gas in an alternating way (20 to 40deg C & 20 psi steps)15. For a water jet of 170deg C at the reservoir the Ar pressure is supposedly ~120 psi16. Feel the Knee with your finger (caution: warm to hot): You likely will feel a temperature gradient which can be moved to the left and

right with increasing the temperature of the reservoir and increasing the gas pressure

Stop the seeded Jet17. Close Vseed and the gas bottle18. See STOP AND START JET IN CHAMBER or STOP ENTIRE LIQUID-TO-GAS JET OPERATION OR MAKE A REFILL19. Open Cexhaust

20. Open Vexhaust slowly to drain the gas (should take 2 to 3 seconds)21. Close Vexhaust

22. Open Vpump and pump for 1 minute23. Close the gas regulator and Vpump 10

STOP ENTIRE LIQUID-TO-GAS JET OPERATION OR MAKE A REFILL

Stop Jet in Chamber1. Close Vseed

2. Close Vblocking

3. Open Vevac-line

4. Open Vthree-way to exhaust slowly (should take 5 seconds)5. Open Vthree-way to pump and pump for 15 seconds, then close Vthree-way again6. Close Vnozzle

Re-transfer Liquid back to Supply Reservoir (for non hazardous liquids only !)7. Close Vblocking

8. Close Vdrain

9. While the Reservoir and the gas line is hot slowly open Vtransfer and monitor the liquid level in the glass funnel. CloseVtransfer when the level stopped rising and no more bubbles make it to the surface.

If your Chemical is hazardous or toxic:10. Do not re-transfer the liquid but open Vevac-line and open Vthree-way to exhaust11. Monitor with the ion-gauges and the COLTRIMS spectrometer if the jet is fading. You can close Vthree-way and check if

the source chamber is falling or rising after a while; if it is still rising there is still liquid – if it is stable or falling you can now pump on it.

12. You may want to heat up the reservoir if it safe to accelerate the process. With 100 deg C it can take 2h for ~100ml.13. Alternatively use Syringe to suck out the reservoir: Open Vsupply, open Vsyringe and pull the plunger as far out as

possible. Close Vsupply, close Vsyringe. Detach syringe (pink nut) and bring it to a fumehood to drain it. Cap Vsupply.

Drain (and refill) the Reservoir13. Stop the reservoir heater, i.e. set the heater to 20degC (not higher !) and monitor the cool-down process. Wait for

the temperate to go down to <30deg C. You may want to use a bucket with water to cool down the reservoir after carefully removing the heater sleeve (caution: hot on the inside).

14. In case you want to refill the reservoir close Vnozzle, open Vblocking and Vevac-line and open Vthree-way to the pump and pump for 20 seconds, then close Vthree-way, Vevac-line and Vblocking and transfer more liquid using the transfer arm or the syringe.

See next page =>11

continue: STOP ENTIRE LIQUID-TO-GAS JET OPERATION OR MAKE A REFILL

In case you DO NOT want to refill:

- Step 1: Clean the gas lines15. Keep Heaters of outside and inside gaslines on16. Close Vblocking

17. Open Vevac-line

18. Open Vthree-way to forepump

19. Pump out as long as you can (>1day if possible)

- Step 2: Pump out the Reservoir20. Make sure Vnozzle is closed21. Wear your PPE (Gloves, Glasses, etc.): Open Creservoir-drain and drain the liquid into a beaker22. Open Cdry-out and attach dry gas with reasonable flow which you can control by opening Vdry-out

23. Open Vevac-line

24. Open Vblocking

25. Close Vthree-way to the pump just a little bit to give some gas ballast; watch for liquid coming out of the pump exhaust

26. Let it run for 2 to 12 hours27. Now detach dry gas and close Vdry-out, Cdry-out and Creservoir-drain. You can now pump out the reservoir by opening

Vthree-way for at least 3 minutes. Optional: Close Vthree-way afterwards, open Vprotect and Vbypass to pump with scroll.

12

CLEAN-UP PROCESS

Clean out the Supply Vessel1. Close Vtransfer

2. Wear your PPE (Gloves, Glasses, etc.): Open Csupply-drain

3. Open Vdrain and empty liquid into a beaker4. Attach a dry gas to Csupply-drain and dial in a decent flow by opening Vdry-out

5. Let it run for 2 to 12 hours

Clean the Syringe1. Wear your PPE (Gloves, Glasses, etc.)2. Empty the syringe in the fume hood by retransferring as much liquid into a beaker as possible3. Note: There is likely still <5ml of liquid in the syringe even if the plunger is all the way in.4. Open the syringe in the fume hood by taking out the plunger back-stop (using a screwdriver to take of

the 6 little screws) and drain all fluids5. Clean syringe with isopropanol using a soaked tissue and long tweezers (note: don’t scratch the

stainless steel surface)6. Use silicon (vacuum) grease to lightly lubricate the two O-rings on the plunger

Regenerate the Forepump(s)In case you polluted the forepumps with any condensable gases open the gas ballasts or detach forepumpand let it pump a small amount of (dry) air, i.e. you need to restrict the flow with either a small pin hole in a Kwik-Flange plastic cap or a screw with a washer in the (red water) hose or similar.

13